CN109181883B - Production process of refined horse oil ethyl ester - Google Patents
Production process of refined horse oil ethyl ester Download PDFInfo
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- CN109181883B CN109181883B CN201811240962.9A CN201811240962A CN109181883B CN 109181883 B CN109181883 B CN 109181883B CN 201811240962 A CN201811240962 A CN 201811240962A CN 109181883 B CN109181883 B CN 109181883B
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
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Abstract
The invention discloses a production process of refined horse oil ethyl ester, which comprises the steps of boiling horse fat, and obtaining crude horse oil after refining treatment; carrying out an ethylation reaction on the crude horse oil to obtain crude horse oil ethyl ester; and refining and purifying the crude horse oil ethyl ester by adopting a thin film evaporation method to obtain refined horse oil ethyl ester. On the premise of reserving rich unsaturated fatty acid of the horse oil, the invention obviously improves the oil yield of the horse oil, the yield of crude horse oil ethyl ester and the yield of refined horse oil ethyl ester, thereby obtaining the refined horse oil ethyl ester with high quality and high yield; and the process flow is simple, the repeatability is good, and the economic value is good.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a production process of refined horse oil ethyl ester.
Background
Horse oil is grease obtained from horse bristles or tail of horse tail, horse abdominal adipose tissue, horse visceral adipose tissue, and horse ridge adipose tissue, and is also called horse fat; a series of post-treatment processes are carried out on extracted horse oil and fat, the post-treatment processes comprise oil extraction and deep processing processes, the oil extraction process comprises decolorization, degumming, deodorization and deacidification, the deep processing process of horse fat comprises the steps of ester exchange, oil fractionation, oil hydrogenation and the like, pure oil can be obtained after the oil is extracted and deeply processed, and the obtained pure oil has important application in the fields of daily chemicals, cosmetics and the like except for edibility.
The quantity of horses in China is large, the horse oil resources are rich and high in quality, and Sinkiang is one of important horse producing bases in China and has a large amount of horse fat resources. According to the statistical data of Xinjiang Uygur autonomous region statistical bureau "Xinjiang statistics New year book 2017", 89.01 ten thousand horses are counted according to the livestock feeding condition by 2016 years, and the number of horses in Kazak autonomous state in Ili reaches 60.97 ten thousand, which accounts for 68% of the total number of horses. Total meat yield in Xinjiang as a horse meat product was 6.17 million tons, and horse meat yield in Ile, Kazak, autonomous State, was 4.64 million tons, accounting for 75% of the total horse meat. According to the results of market research, the total horse fat yield in Xinjiang in 2016 is about 1760 tons calculated according to that the meat-oil ratio of horses is close to 35: 1. Sinkiang has good natural conditions and resource advantages, but horse oil is rarely developed and utilized, and the horse oil in Sinkiang is mainly sold to Korea, Japan and other regions in the form of cheap primary raw materials as the primary raw material of horse oil cosmetics due to the absence of horse oil refining and processing technology, so that the development and utilization of a simple and efficient process for refining, esterifying and refining the horse oil is urgent, and the process has great significance for the development of horse oil daily chemical products and cosmetics in China and Sinkiang.
The method for refining the animal fat mainly comprises the following steps: squeezing, alkali hydrolysis, solvent extraction, decocting, steaming, biological enzymolysis, membrane separation, supercritical extraction, and microwave-assisted extraction. The oil refining process generally comprises alkali refining, acid pickling, decoloration and the like.
Chinese patent CN1078490A discloses a method for producing refined horse oil, which uses a boiling method process, the first step is boiling horse bristles, horse tails and subcutaneous fat thereof with water or heating the horse bristles, horse tails and subcutaneous fat thereof to 80-90 ℃ for hours by introducing steam, then standing the horse bristles, horse tails and subcutaneous fat to separate out upper-layer grease, thus obtaining crude horse oil; the second step is to add alkali to neutralize to pH 7 and then wash with water. And thirdly, removing odor by steam stripping, decoloring by a decoloring agent (mixing active carbon, active clay and diatomite), filtering, standing, layering and dehydrating to obtain the refined horse oil. The method is simple and practical, and the operation conditions are easy to control, but crude fat combined with protein, connective tissue, skin, tendon and the like can not be effectively separated from impurities, so that the extraction rate of the horse oil is low, and meanwhile, the obtained horse oil is affected by oxidation and deterioration of unsaturated fatty acid due to the addition of external water for cooking.
Chinese invention patent CN1456648A discloses a horse fat extraction and industrial application, in the method of the invention, horse fat tissue is collected, crude horse fat and refined horse fat are extracted, and the method is applied to the industrial production of various products. The horse fat extraction method mentioned in this patent comprises: extruding and puffing pretreatment, adding water for pretreatment, extracting by an organic solvent, extracting by supercritical fluid, refining by molecular distillation, refining by ultrasonic treatment, refining by microwave treatment, refining by alkali, refining by steam, and decoloring refined horse fat; the horse fat industrial application comprises: horse fat encapsulation, soap and detergent manufacture, paints and inks, leather processing and care, textile processing, skin care and care, cosmetics. The practical operability and repeatability of the patented method is not high.
Chinese invention patent CN201310346173.4 discloses an unsaturated fatty acid-rich grease and a preparation method thereof, the specific preparation method comprises: firstly, smashing horse fat to obtain liquid grease under the heating condition; secondly, mixing the horse oil and the saponifying agent according to the mass ratio to obtain saponified liquid; thirdly, washing and extracting the saponified solution, and obtaining the horse oil mixed fatty acid by acid washing; and fourthly, carrying out solvent crystallization according to different crystallization temperatures of components in the horse oil, and further separating to obtain unsaturated fatty acid which comprises oleic acid, linoleic acid, linolenic acid and palmitoleic acid. The process of this patent is very complicated, and the horse oil is first converted from triglyceride form into fatty acid soap for extraction, then acidified with a large amount of strong acid to be converted into fatty acid, and extracted again with organic solvent. The process not only needs a large amount of strong acid (hydrochloric acid and sulfuric acid) and strong base (sodium hydroxide), but also needs a large amount of organic solvent, and the process of removing the solvent after extraction has high solvent consumption and high energy consumption, so the method has high cost on the whole, generates waste water and waste liquid which are easy to cause environmental pollution, and most importantly, the obtained end product is in a fatty acid form and cannot be directly applied to food and cosmetics.
Chinese invention patent CN104974857A discloses a preparation method of an ethylated horse oil and horse oil thereof, the invention adds alcohol and alkali catalyst into crude horse oil to carry out ethylation reaction, after the reaction is finished, the mixture of glycerol and fatty acid ethyl ester is centrifuged, and the upper layer oil is taken to obtain the refined horse oil. The invention avoids the oxidation of unsaturated fatty acid in horse oil in the heating and boiling process, thereby retaining the rich unsaturated fatty acid of horse oil to the maximum extent, effectively reducing the melting boiling point of the unsaturated fatty acid and having stable state. However, when the method is actually repeated, the invention discovers that the collected crude horse oil is not primarily refined but is directly processed by the ethylation of the horse oil by the alkali catalytic alcoholysis method, so that various impurities are difficult to separate from the horse fat, the horse fat can be combined with impurities such as protein, connective tissues, skins, tendons and the like, and the impurities wrap and associate the horse oil, so that the horse oil and the impurities cannot be effectively separated, the reactivity of the horse oil is greatly hindered, and the impurities can also influence the esterification reaction.
The horse oil extracting process with enzymolysis process includes the following steps: fresh horse fat, impurity removal, cleaning, chopping, adding distilled water, adjusting the pH value, adding enzyme, performing water bath enzymolysis, centrifuging, taking upper-layer grease to obtain crude horse oil, and optimizing an extraction company by a single-factor experiment and an orthogonal experiment method to obtain the optimal extraction process: the enzymolysis temperature is 55 ℃, the enzymolysis time is 2.5h, the enzyme addition amount is 1%, the pH value is 6.5, and the horse oil extraction rate is 74.74%. [ Zhengjing, Houweiwei, Zhuyun, Zhengyunfen, Populi swallow ] and horse oil extraction technology research by enzymolysis method [ J]Chinese food and nutrition, 2013,19(11):55-58.]. Subsequently, supercritical CO was investigated2Horse fat is extracted by fluid, and through Box-Behnken software design experiments, optimal technological parameters are obtained through optimization, wherein the optimal technological parameters are extraction pressure of 32MPa, extraction temperature of 39 ℃, extraction time of 5 hours, and oil yield of the horse fat is 72.96%. Supercritical CO of Wanwenjun2Study of the rheological Properties and storage qualities of the margarines obtained by fluid extraction [ D]Sinkiang university of agriculture, 2016.]. The two methods have complex extraction process and high cost, and are not easy to realize large-scale industrial production and application.
Therefore, summarizing the existing processes, it can be found that the main reason for the development resistance of horse oil products is the immaturity of the complete process of refining, esterifying and refining horse oil. Therefore, a simple, efficient, operable and repeatable refining and esterifying process for refining horse oil is urgently needed to be developed and utilized, and the core of the process needs to be solved to improve the oil yield of crude horse oil in the refining process, and ensure the purity and high quality of a terminal product, namely horse oil ethyl ester.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provide a production process of refined horse oil ethyl ester, which can obviously improve the oil yield of horse oil, the yield of crude horse oil ethyl ester and the yield of refined horse oil ethyl ester on the premise of keeping rich unsaturated fatty acid of horse oil, thereby obtaining the refined horse oil ethyl ester with high quality and high yield.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a production process of refined horse oil ethyl ester is characterized by comprising the following steps:
a. boiling horse fat, and refining to obtain crude horse oil;
b. carrying out an ethylation reaction on the crude horse oil to obtain crude horse oil ethyl ester;
c. and refining and purifying the crude horse oil ethyl ester by adopting a thin film evaporation method to obtain refined horse oil ethyl ester.
Preferably, the boiling of horse fat in the step a is as follows: stirring and crushing horse fat at room temperature, adding the horse fat into a reaction kettle, heating to 80-120 ℃, stirring for 4-5 hours, and vacuumizing and dehydrating a reaction product at 100-120 ℃.
Preferably, the refining process in step a is as follows: after the reaction product is vacuumized and dehydrated, filtering the reaction product twice at 80-100 ℃, firstly filtering the reaction product for the first time by using a filter screen, and collecting the clear liquid of horse oil grease; and then filtering the horse oil grease clear liquid for the second time by using filter cloth of 250-300 meshes, and collecting a filtering product to obtain crude horse oil.
Preferably, in the step b, a vertical condenser and a circulating water pump are opened, the crude horse oil, absolute ethyl alcohol and alkali are added into an esterification reaction kettle according to the weight ratio of 200: 80-85: 1.0-1.4, the mixture is stirred and heated to 70-72 ℃ for esterification reaction for 6-7 hours, then the vertical condenser is closed, the stirring and heating are stopped, and the crude horse oil ethyl ester is obtained after standing.
Preferably, in the step b, absolute ethyl alcohol and alkali are sequentially added into the esterification reaction kettle, the mixture is heated and stirred, the alkali is completely dissolved in the absolute ethyl alcohol, and then crude horse oil is added.
Preferably, in the step b, after the esterification reaction is completed, the vertical condenser is closed, the horizontal condenser is opened, and the anhydrous ethanol is recovered at 70-72 ℃ by a reduced pressure distillation method.
Preferably, in the step c, the crude horse oil ethyl ester is added into a heavy component kettle, the temperature is controlled to be 210-220 ℃ under the vacuum condition, a thin film evaporator is adopted for evaporation to refine the horse oil ethyl ester, the refined horse oil ethyl ester enters a light component kettle, and nitrogen is introduced for protection.
Still more preferably, in said step c, crude horse oil ethyl ester is added to 2/3 of the heavies kettle volume.
Firstly, stirring collected horse fat, and destroying tissues and cells by mechanical action to release grease; then, the crude horse oil is refined by wet boiling, in the wet boiling process, no external moisture is added, the crude horse oil is heated under the condition that moisture exists in the horse fat, the oil yield of the horse oil is high and can reach more than 78 percent, the horse oil is light in color and free of obvious peculiar smell, and rich unsaturated fatty acid of the horse oil can be reserved; then a filter screen and filter cloth are used for sequentially carrying out hot filtration on the horse fat decocted by the wet method, so that the horse oil is well separated from impurities such as skin, muscle, connective tissue, muscle and the like; the crude horse oil after being refined and filtered can be directly subjected to effective ethyl esterification reaction. The ethyl alcohol is used as a solvent and a reactant, the alkali is used as a catalyst, the refined crude horse oil is subjected to an ethylation reaction, conditions such as material proportion, reaction temperature and the like in the reaction are optimized, and the yield of the crude horse oil ethyl ester is remarkably improved to over 95%. And finally, purifying the crude horse oil ethyl ester by adopting a film evaporation method, wherein the film evaporation method is high in vacuum degree, low in operation temperature, short in heating time and high in evaporation efficiency, and the yield of refined horse oil ethyl ester is effectively improved to be more than 90%.
The invention has the following beneficial effects: on the premise of reserving rich unsaturated fatty acid of the horse oil, the invention obviously improves the oil yield of the horse oil, the yield of crude horse oil ethyl ester and the yield of refined horse oil ethyl ester, thereby obtaining the refined horse oil ethyl ester with high quality and high yield; and the process flow is simple, the repeatability is good, and the economic value is good.
Drawings
FIG. 1 is a GC-MS (gas-mass spectrometry) total ion flow spectrum of refined horse oil ethyl ester according to the invention.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
Example 1
Refining the crude horse oil: at room temperature, fresh horse fat is crushed by a meat grinder, then the horse fat is added into a stainless steel reaction kettle, the mixture is heated to 80 ℃, stirred for 4 hours, a vent valve is opened to release partial water vapor, a horizontal condensation switch is opened, vacuum dehydration is carried out at 100 ℃ until no water drops in a water separator, then primary filtration is carried out by a stainless steel filter screen at 80 ℃, the horse fat clear liquid is collected, secondary filtration is carried out on the clear liquid by a filter cloth with 250 meshes, and the filtration product is collected to obtain crude horse oil, wherein the oil yield is 78.7%.
Esterification of crude horse oil: firstly, 3 kilograms of absolute ethyl alcohol is added into a stainless steel barrel, 1.0 kilogram of caustic soda is added into the stainless steel barrel, a wood bar is used for rolling and stirring to dissolve the caustic soda, the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into an esterification reaction kettle, if the barrel contains no molten caustic soda, the 3 kilograms of absolute ethyl alcohol is added into the barrel, the wood bar is used for rolling and stirring to dissolve the caustic soda, and the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into the esterification reaction kettle. Closing a switch of the horizontal condenser, opening a switch of the vertical condenser, opening a circulating water pump, adding 72 kg of absolute ethyl alcohol (about 80 kg of absolute ethyl alcohol for dissolving caustic soda in total) into the esterification reaction kettle, closing a cover of the esterification reaction kettle, heating to 40 ℃, and stirring to ensure that the caustic soda is completely and well dissolved in the absolute ethyl alcohol.
Adding 200 kg of refined crude horse oil into an esterification reaction kettle, stirring, and heating to 70 ℃ for esterification reaction for 6 hours. After the reaction is finished, closing the vertical condensation switch and opening the horizontal condensation switch; distilling out ethanol, recovering ethanol from the recovering tank under reduced pressure when ethanol is not refluxed at 70 deg.C, and recovering ethanol from the recovering tank under reduced pressure. Stopping stirring and heating, standing for 15 hours, then opening a valve at the bottom of the esterification reaction kettle, and discharging the lower layer of glycerol. The glycerol is in a syrup shape, has high viscosity and flows down from a valve in a strand manner; the crude horse oil ethyl ester on the upper layer has smaller viscosity and is left in a spraying state from a valve, so that whether the glycerol is completely put can be judged, and the yield of the horse oil ethyl ester is 94.8%.
Refining crude horse oil ethyl ester: adding crude horse oil ethyl ester into a heavy component kettle; crude ethyl maleate was added at 2/3 volumes to the heavies kettle. Then opening a vacuum system switch and a material pipe switch, controlling the temperature at 210 ℃, carrying out evaporation condensation in an evaporator for mutual reaction, wherein the reaction time needs to be determined according to the condition that the horse oil ethyl ester product is sampled, refined horse oil ethyl ester product enters a light component kettle, two light component kettles are counted, and one kettle is filled and then the next kettle is installed; the yield of the refined horse oil ethyl ester obtained after the thin film evaporation reaches 90.0 percent, and the refined horse oil ethyl ester product is stored by introducing nitrogen.
Example 2
Refining the crude horse oil: at room temperature, fresh horse fat is crushed by a meat grinder, then the horse fat is added into a stainless steel reaction kettle, the mixture is heated to 120 ℃, stirred for 5 hours, a vent valve is opened to release partial water vapor, a horizontal condensation switch is opened, vacuum dehydration is carried out at 120 ℃ until no water drops in a water separator, then primary filtration is carried out at 90 ℃ by a stainless steel filter screen, horse fat clear liquid is collected, secondary filtration is carried out on the clear liquid by 250-mesh filter cloth, and a filtration product is collected to obtain crude horse oil, wherein the oil yield is 79.1%.
Esterification of crude horse oil: firstly, 3 kilograms of absolute ethyl alcohol is added into a stainless steel barrel, 1.1 kilograms of caustic soda is added into the stainless steel barrel, a wood bar is used for rolling and stirring to dissolve the caustic soda, the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into an esterification reaction kettle, if the barrel contains no molten caustic soda, 3 kilograms of absolute ethyl alcohol is added into the barrel, the wood bar is used for rolling and stirring to dissolve the caustic soda, and the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into the esterification reaction kettle. Closing a switch of the horizontal condenser, opening a switch of the vertical condenser, opening a circulating water pump, adding 72 kg of absolute ethyl alcohol (about 80 kg of absolute ethyl alcohol for dissolving caustic soda in total) into the esterification reaction kettle, closing a cover of the esterification reaction kettle, heating to 40 ℃, and stirring to ensure that the caustic soda is completely and well dissolved in the absolute ethyl alcohol.
Adding 200 kg of refined crude horse oil into an esterification reaction kettle, stirring, and heating to 72 ℃ for esterification reaction for 7 hours. After the reaction is finished, closing the vertical condensation switch and opening the horizontal condensation switch; distilling out ethanol, recovering ethanol from the recovering tank under reduced pressure when ethanol is not refluxed at 72 deg.C, and recovering ethanol from the recovering tank under reduced pressure. Stopping stirring and heating, standing for 15 hours, then opening a valve at the bottom of the esterification reaction kettle, and discharging the lower layer of glycerol. The glycerol is in a syrup shape, has high viscosity and flows down from a valve in a strand manner; the viscosity of the ethyl ester at the upper layer is small, and the ethyl ester is left in a spraying state from a valve, so that whether the glycerol is completely put can be judged, and the yield of the esterification of the horse oil is 95.5%.
Refining crude horse oil ethyl ester: adding crude horse oil ester obtained by esterification into a heavy component kettle; crude ethyl maleate was added at 2/3 volumes to the heavies kettle. And then a vacuum system switch and a material pipe switch are opened, the temperature is controlled at 213 ℃, evaporation and condensation are carried out in the evaporator to carry out mutual reaction, and the reaction time needs to be determined according to the condition of the output of the horse oil ethyl ester product. Feeding the refined horse oil ethyl ester product into a light component kettle, wherein the total amount of the light component kettle is two, and one kettle is filled with the refined horse oil ethyl ester product and then the other kettle is filled with the refined horse oil ethyl ester product; the yield of the refined horse oil ethyl ester obtained after the thin film evaporation reaches 92.6 percent, and the refined horse oil ethyl ester product is stored by introducing nitrogen.
Example 3
Refining the crude horse oil: at room temperature, fresh horse fat is crushed by a meat grinder, then the crushed horse fat is added into a stainless steel reaction kettle, the stainless steel reaction kettle is heated to 120 ℃, the stirring is carried out for 4 hours, a vent valve is opened to release partial water vapor, a horizontal condensation switch is opened, the vacuum dehydration is carried out at 110 ℃ until no water drops in a water separator, then the stainless steel filter screen is firstly used for primary filtration at 80 ℃, the horse fat clear liquid is collected, the clear liquid is secondarily filtered by 300-mesh filter cloth, the filtration product is collected, the crude horse oil is obtained, and the oil yield is 78.9%.
Esterification of crude horse oil: firstly, 3 kilograms of absolute ethyl alcohol is added into a stainless steel barrel, 1.2 kilograms of caustic soda is added into the stainless steel barrel, a wood bar is used for rolling and stirring to dissolve the caustic soda, the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into an esterification reaction kettle, if the barrel contains no molten caustic soda, the 3 kilograms of absolute ethyl alcohol is added into the barrel, the wood bar is used for rolling and stirring to dissolve the caustic soda, and the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into the esterification reaction kettle. Closing a switch of the horizontal condenser, opening a switch of the vertical condenser, opening a circulating water pump, adding 75 kg of absolute ethyl alcohol (about 85 kg of absolute ethyl alcohol for dissolving caustic soda in total) into the esterification reaction kettle, closing a cover of the esterification reaction kettle, heating to 40 ℃, and stirring to ensure that the caustic soda is completely and well dissolved in the absolute ethyl alcohol.
200 kg of horse oil is added into an esterification reaction kettle, stirred and heated to 72 ℃ for esterification reaction for 7 hours. After the reaction is finished, closing the vertical condensation switch and opening the horizontal condensation switch; distilling ethanol, recovering ethanol from the recovering tank, and recovering ethanol from the recovering tank by vacuum distillation when ethanol is not refluxed at 70-72 deg.C until ethanol is dried under reduced pressure. Stopping stirring and heating, standing for 15 hours, then opening a valve at the bottom of the esterification reaction kettle, and discharging the lower layer of glycerol. The glycerol is in a syrup shape, has high viscosity and flows down from a valve in a strand manner; the viscosity of the ethyl ester at the upper layer is small, and the ethyl ester is left in a spraying state from a valve, so that whether the glycerol is completely put can be judged, and the yield of the esterification of the horse oil is 95.8%.
Refining crude horse oil ethyl ester: adding crude horse oil ester obtained by esterification into a heavy component kettle; crude ethyl maleate was added at 2/3 volumes to the heavies kettle. And then opening a vacuum system switch and a material pipe switch, controlling the temperature at 215 ℃, carrying out evaporation condensation in the evaporator, and carrying out mutual reaction, wherein the reaction time needs to be the condition that the horse oil ethyl ester product is sampled. Feeding the refined horse oil ethyl ester product into a light component kettle, wherein the total amount of the light component kettle is two, and one kettle is filled with the refined horse oil ethyl ester product and then the other kettle is filled with the refined horse oil ethyl ester product; the yield of refined horse oil ethyl ester obtained after thin film evaporation reaches 91.3%, and the refined horse oil ethyl ester product is stored by introducing nitrogen.
Example 4
Refining the crude horse oil: at room temperature, mincing fresh horse fat by using a meat mincer, adding the minced horse fat into a stainless steel reaction kettle, heating to 120 ℃, stirring for 5 hours, opening an air release valve to release partial water vapor, opening a horizontal condensation switch, vacuumizing and dehydrating at 120 ℃ until water knockout drum does not drip any more, primarily filtering by using a stainless steel filter screen at 80 ℃, collecting horse fat clear liquid, secondarily filtering the clear liquid by using filter cloth of 250-300 meshes, collecting a filtering product, and obtaining crude horse oil, wherein the oil yield is 79.6%.
Esterification of crude horse oil: firstly, 3 kilograms of absolute ethyl alcohol is added into a stainless steel barrel, 1.3 kilograms of caustic soda is added into the stainless steel barrel, a wood bar is used for rolling and stirring to dissolve the caustic soda, the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into an esterification reaction kettle, if the barrel contains no molten caustic soda, 3 kilograms of absolute ethyl alcohol is added into the barrel, the wood bar is used for rolling and stirring to dissolve the caustic soda, and the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into the esterification reaction kettle. Closing a switch of the horizontal condenser, opening a switch of the vertical condenser, opening a circulating water pump, adding 75 kg of absolute ethyl alcohol (about 80 kg of absolute ethyl alcohol for dissolving caustic soda), closing a cover of the esterification reaction kettle, heating to 40 ℃, and stirring to ensure that the caustic soda is completely and well dissolved in the absolute ethyl alcohol.
200 kg of horse oil is added into an esterification reaction kettle, stirred and heated to 72 ℃ for esterification reaction for 6 hours. After the reaction is finished, closing the vertical condensation switch and opening the horizontal condensation switch; distilling out ethanol, recovering ethanol from the recovering tank under reduced pressure when ethanol is not refluxed at 72 deg.C, and recovering ethanol from the recovering tank under reduced pressure. Stopping stirring and heating, standing for 15 hours, then opening a valve at the bottom of the esterification reaction kettle, and discharging the lower layer of glycerol. The glycerol is in a syrup shape, has high viscosity and flows down from a valve in a strand manner; the viscosity of the ethyl ester at the upper layer is small, and the ethyl ester is left in a spraying state from a valve, so that whether the glycerol is completely put can be judged, and the yield of the esterification of the horse oil is 96.1%.
Refining crude horse oil ethyl ester: adding crude horse oil ester obtained by esterification into a heavy component kettle; when the materials are added, the amount of the materials added is proper at the heavy component kettle 2/3. And then opening a vacuum system switch and a material pipe switch, controlling the temperature at 217 ℃, carrying out evaporation condensation in the evaporator for mutual reaction, wherein the reaction time needs to be determined according to the condition of the output of the horse oil ethyl ester product. The horse oil ethyl ester product enters a light component kettle, and two light component kettles are arranged in total, wherein one kettle is filled with the light component kettle and then the other kettle is arranged; the yield of the horse oil ethyl ester obtained after film evaporation reaches 92.8 percent, and the horse oil ethyl ester product is stored by introducing nitrogen.
Example 5
Refining the crude horse oil: at room temperature, fresh horse fat is crushed by a meat grinder, then the crushed horse fat is added into a stainless steel reaction kettle, the stainless steel reaction kettle is heated to 120 ℃, the stirring is carried out for 4 hours, a vent valve is opened to release partial water vapor, a horizontal condensation switch is opened, the vacuum dehydration is carried out at 100 ℃ until no water drops in a water separator, then the stainless steel filter screen is firstly used for primary filtration at 100 ℃, the horse fat clear liquid is collected, the clear liquid is secondarily filtered by a 250-mesh filter cloth, the filtration product is collected, the crude horse oil is obtained, and the oil yield is 78.7%.
Esterification of crude horse oil: firstly, 3 kilograms of absolute ethyl alcohol is added into a stainless steel barrel, 1.3 kilograms of potassium hydroxide is added into the stainless steel barrel, a wood bar is used for rolling and stirring to dissolve alkali, the ethyl alcohol with the potassium hydroxide dissolved in the barrel is carefully poured into an esterification reaction kettle, if the potassium hydroxide which is not melted exists in the barrel, the 3 kilograms of absolute ethyl alcohol is added into the barrel, the wood bar is used for rolling and stirring to dissolve alkali, and the ethyl alcohol with the potassium hydroxide dissolved in the barrel is carefully poured into the esterification reaction kettle. Closing a switch of the horizontal condenser, opening a switch of the vertical condenser, opening a circulating water pump, adding 72 kg of absolute ethyl alcohol (about 80 kg of absolute ethyl alcohol for dissolving potassium hydroxide in total) into the esterification reaction kettle, closing a cover of the esterification reaction kettle, heating to 40 ℃, and stirring to ensure that the potassium hydroxide is completely and well dissolved in the absolute ethyl alcohol.
200 kg of horse oil is added into an esterification reaction kettle, stirred and heated to 72 ℃ for esterification reaction for 7 hours. After the reaction is finished, closing the vertical condensation switch and opening the horizontal condensation switch; distilling out ethanol, recovering ethanol from the recovering tank under reduced pressure when ethanol is not refluxed at 72 deg.C, and recovering ethanol from the recovering tank under reduced pressure. Stopping stirring and heating, standing for 15 hours, then opening a valve at the bottom of the esterification reaction kettle, and discharging the lower layer of glycerol. The glycerol is in a syrup shape, has high viscosity and flows down from a valve in a strand manner; the viscosity of the ethyl ester at the upper layer is small, and the ethyl ester is left in a spraying state from a valve, so that whether the glycerol is completely put can be judged, and the yield of the esterification of the horse oil is 95.1%.
Refining crude horse oil ethyl ester: adding crude horse oil ester obtained by esterification into a heavy component kettle; when the materials are added, the amount of the materials added is proper at the heavy component kettle 2/3. And then, opening a vacuum system switch and a material pipe switch, controlling the temperature at 220 ℃, carrying out evaporation condensation in an evaporator, and carrying out mutual reaction, wherein the reaction time needs to be determined according to the condition of the output of the horse oil ethyl ester product. The horse oil ethyl ester product enters a light component kettle, and two light component kettles are arranged in total, wherein one kettle is filled with the light component kettle and then the other kettle is arranged; the yield of the horse oil ethyl ester obtained after film evaporation reaches 90.4%, and the horse oil ethyl ester product is stored by introducing nitrogen.
Example 6
Refining the crude horse oil: at room temperature, fresh horse fat is crushed by a meat grinder, then the crushed horse fat is added into a stainless steel reaction kettle, the stainless steel reaction kettle is heated to 120 ℃, the stirring is carried out for 5 hours, a vent valve is opened to release partial water vapor, a horizontal condensation switch is opened, vacuum dehydration is carried out at 120 ℃ until no water drops in a water separator, then primary filtration is carried out by a stainless steel filter screen at 100 ℃, horse fat clear liquid is collected, secondary filtration is carried out on the clear liquid by a filter cloth with 250 meshes, and a filtration product is collected to obtain crude horse oil, wherein the oil yield is 77.8%.
Esterification of crude horse oil: firstly, 3 kilograms of absolute ethyl alcohol is added into a stainless steel barrel, 1.3 kilograms of caustic soda is added into the stainless steel barrel, a wood bar is used for rolling and stirring to dissolve the caustic soda, the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into an esterification reaction kettle, if the barrel contains no molten caustic soda, 3 kilograms of absolute ethyl alcohol is added into the barrel, the wood bar is used for rolling and stirring to dissolve the caustic soda, and the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into the esterification reaction kettle. Closing a switch of the horizontal condenser, opening a switch of the vertical condenser, opening a circulating water pump, adding 72 kg of absolute ethyl alcohol (about 80 kg of absolute ethyl alcohol for dissolving caustic soda in total) into the esterification reaction kettle, closing a cover of the esterification reaction kettle, heating to 40 ℃, and stirring to ensure that the caustic soda is completely and well dissolved in the absolute ethyl alcohol.
200 kg of horse oil is added into an esterification reaction kettle, stirred and heated to 71 ℃ for esterification reaction for 6 hours. After the reaction is finished, closing the vertical condensation switch and opening the horizontal condensation switch; distilling out ethanol, recovering ethanol from the recovering tank under reduced pressure when ethanol is not refluxed at 71 deg.C, and recovering ethanol from the recovering tank under reduced pressure until ethanol is dried. Stopping stirring and heating, standing for 15 hours, then opening a valve at the bottom of the esterification reaction kettle, and discharging the lower layer of glycerol. The glycerol is in a syrup shape, has high viscosity and flows down from a valve in a strand manner; the viscosity of the ethyl ester at the upper layer is small, and the ethyl ester is left in a spraying state from a valve, so that whether the glycerol is completely put can be judged, and the yield of the esterification of the horse oil is 94.5%.
Refining crude horse oil ethyl ester: adding crude horse oil ester obtained by esterification into a heavy component kettle; when the materials are added, the amount of the materials added is proper at the heavy component kettle 2/3. And then, opening a vacuum system switch and a material pipe switch, controlling the temperature at 220 ℃, carrying out evaporation condensation in an evaporator, and carrying out mutual reaction, wherein the reaction time needs to be determined according to the condition of the output of the horse oil ethyl ester product. The horse oil ethyl ester product enters a light component kettle, and two light component kettles are arranged in total, wherein one kettle is filled with the light component kettle and then the other kettle is arranged; the yield of the horse oil ethyl ester obtained after film evaporation reaches 91.1 percent, and the horse oil ethyl ester product is stored by introducing nitrogen.
Example 7
Refining the crude horse oil: at room temperature, mincing fresh horse fat by using a meat mincer, adding the minced horse fat into a stainless steel reaction kettle, heating to 120 ℃, stirring for 5 hours, opening an air release valve to release partial water vapor, opening a horizontal condensation switch, vacuumizing and dehydrating at 120 ℃ until water knockout drum does not drip any more, primarily filtering by using a stainless steel filter screen at 90 ℃, collecting horse fat clear liquid, secondarily filtering the clear liquid by using filter cloth of 250-30 meshes, collecting a filtering product, and obtaining crude horse oil, wherein the oil yield is 78.4%.
Esterification of crude horse oil: firstly, 3 kilograms of absolute ethyl alcohol is added into a stainless steel barrel, 1.3 kilograms of caustic soda is added into the stainless steel barrel, a wood bar is used for rolling and stirring to dissolve the caustic soda, the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into an esterification reaction kettle, if the barrel contains no molten caustic soda, 3 kilograms of absolute ethyl alcohol is added into the barrel, the wood bar is used for rolling and stirring to dissolve the caustic soda, and the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into the esterification reaction kettle. Closing a switch of the horizontal condenser, opening a switch of the vertical condenser, opening a circulating water pump, adding 73 kg of absolute ethyl alcohol (about 82 kg of absolute ethyl alcohol for dissolving caustic soda in total) into the esterification reaction kettle, closing a cover of the esterification reaction kettle, heating to 40 ℃, and stirring to ensure that the caustic soda is completely and well dissolved in the absolute ethyl alcohol.
200 kg of horse oil is added into an esterification reaction kettle, stirred and heated to 72 ℃ for esterification reaction for 7 hours. After the reaction is finished, closing the vertical condensation switch and opening the horizontal condensation switch; distilling out ethanol, recovering ethanol from the recovering tank under reduced pressure when ethanol is not refluxed at 72 deg.C, and recovering ethanol from the recovering tank under reduced pressure. Stopping stirring and heating, standing for 15 hours, then opening a valve at the bottom of the esterification reaction kettle, and discharging the lower layer of glycerol. The glycerol is in a syrup shape, has high viscosity and flows down from a valve in a strand manner; the viscosity of the ethyl ester at the upper layer is small, and the ethyl ester is left in a spraying state from a valve, so that whether the glycerol is completely put can be judged, and the yield of the esterification of the horse oil is 95.9%.
Refining crude horse oil ethyl ester: adding crude horse oil ester obtained by esterification into a heavy component kettle; when the materials are added, the amount of the materials added is proper at the heavy component kettle 2/3. And then opening a vacuum system switch and a material pipe switch, controlling the temperature at 210-220 ℃, carrying out evaporation condensation in the evaporator for mutual reaction, and observing the condition of the output of the horse oil ethyl ester product when the reaction time is short. The horse oil ethyl ester product enters a light component kettle, and two light component kettles are arranged in total, wherein one kettle is filled with the light component kettle and then the other kettle is arranged; the yield of the horse oil ethyl ester obtained after film evaporation reaches 91.8%, and the horse oil ethyl ester product is stored by introducing nitrogen.
Example 8
Refining the crude horse oil: at room temperature, fresh horse fat is crushed by a meat grinder, then the crushed horse fat is added into a stainless steel reaction kettle, the stainless steel reaction kettle is heated to 120 ℃, the stirring is carried out for 5 hours, a vent valve is opened to release partial water vapor, a horizontal condensation switch is opened, the vacuum dehydration is carried out at 110 ℃ until no water drops in a water separator, then at 90 ℃, the stainless steel filter screen is firstly used for primary filtration, horse fat clean liquid is collected, the clean liquid is secondarily filtered by 250-mesh filter cloth, and a filtration product is collected to obtain crude horse oil, wherein the oil yield is 79.4%.
Esterification of crude horse oil: firstly, 3 kilograms of absolute ethyl alcohol is added into a stainless steel barrel, 1.4 kilograms of caustic soda is added into the stainless steel barrel, a wood bar is used for rolling and stirring to dissolve the caustic soda, the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into an esterification reaction kettle, if the barrel contains no molten caustic soda, the 3 kilograms of absolute ethyl alcohol is added into the barrel, the wood bar is used for rolling and stirring to dissolve the caustic soda, and the ethyl alcohol with the caustic soda dissolved in the barrel is carefully poured into the esterification reaction kettle. Closing a switch of the horizontal condenser, opening a switch of the vertical condenser, opening a circulating water pump, adding 72 kg of absolute ethyl alcohol (about 80 kg of absolute ethyl alcohol for dissolving caustic soda in total) into the esterification reaction kettle, closing a cover of the esterification reaction kettle, heating to 40 ℃, and stirring to ensure that the caustic soda is completely and well dissolved in the absolute ethyl alcohol.
200 kg of horse oil is added into an esterification reaction kettle, stirred and heated to 70 ℃ for esterification reaction for 6 hours. After the reaction is finished, closing the vertical condensation switch and opening the horizontal condensation switch; distilling out ethanol, recovering ethanol from the recovering tank under reduced pressure when ethanol is not refluxed at 70 deg.C, and recovering ethanol from the recovering tank under reduced pressure. Stopping stirring and heating, standing for 15 hours, then opening a valve at the bottom of the esterification reaction kettle, and discharging the lower layer of glycerol. The glycerol is in a syrup shape, has high viscosity and flows down from a valve in a strand manner; the viscosity of the ethyl ester at the upper layer is small, and the ethyl ester is left in a spraying state from a valve, so that whether the glycerol is completely put can be judged, and the yield of the esterification of the horse oil is 95.3%.
Refining crude horse oil ethyl ester: adding crude horse oil ester obtained by esterification into a heavy component kettle; when the materials are added, the amount of the materials added is proper at the heavy component kettle 2/3. And then, opening a vacuum system switch and a material pipe switch, controlling the temperature at 220 ℃, carrying out evaporation condensation in an evaporator, and carrying out mutual reaction, wherein the reaction time needs to be determined according to the condition of the output of the horse oil ethyl ester product. The horse oil ethyl ester product enters a light component kettle, and two light component kettles are arranged in total, wherein one kettle is filled with the light component kettle and then the other kettle is arranged; the yield of the horse oil ethyl ester obtained after film evaporation reaches 92.8 percent, and the horse oil ethyl ester product is stored by introducing nitrogen.
The refined horse oil ethyl ester prepared according to the method of example 1 of the present invention was subjected to GC-MS analysis, and the obtained total ion flow spectrum is shown in fig. 1.
The main peaks in fig. 1 were qualitatively analyzed, and the relative content of each substance was obtained according to the peak area, and the specific analysis is shown in table 1.
Table 1: detection result of components of horse oil ethyl ester
The physical and chemical index test of the refined horse oil ethyl ester sample obtained by the method of example 1 is carried out according to the national standard, the results are shown in table 2, and the physical and chemical index test results show that the acid value and the peroxide value of the product both accord with the edible animal and vegetable oil sanitation standard.
Table 2: results of measuring physical and chemical indexes of horse oil
The present specification and figures are to be regarded as illustrative rather than restrictive, and it is intended that all such alterations and modifications that fall within the true spirit and scope of the invention, and that all such modifications and variations are included within the scope of the invention as determined by the appended claims without the use of inventive faculty.
Claims (4)
1. A production process of refined horse oil ethyl ester is characterized by comprising the following steps:
a. boiling horse fat, and refining to obtain crude horse oil;
b. carrying out an ethylation reaction on the crude horse oil to obtain crude horse oil ethyl ester;
c. refining and purifying the crude horse oil ethyl ester by adopting a thin film evaporation method to obtain refined horse oil ethyl ester;
the process for boiling horse fat in the step a is as follows: stirring horse fat at room temperature, adding into a reaction kettle, heating to 80-120 ℃, stirring for 4-5 hours, and vacuumizing and dehydrating a reaction product at 100-120 ℃; after the reaction product is vacuumized and dehydrated, filtering the reaction product twice at 80-100 ℃, firstly filtering the reaction product for the first time by using a filter screen, and collecting the clear liquid of horse oil grease; filtering the horse oil grease clear liquid for the second time by using filter cloth of 250-300 meshes, and collecting a filtering product to obtain crude horse oil;
in the step b, a vertical condenser and a circulating water pump are opened, crude horse oil, absolute ethyl alcohol and alkali are added into an esterification reaction kettle according to the weight ratio of 200: 80-85: 1.0-1.4, the mixture is stirred and heated to 70-72 ℃ for esterification reaction for 6-7 hours, then the vertical condenser is closed, the stirring and heating are stopped, and the mixture is stood to obtain crude horse oil ethyl ester;
and c, adding the crude horse oil ethyl ester into a heavy component kettle, controlling the temperature to be 210-220 ℃ under a vacuum condition, refining the horse oil ethyl ester by adopting a thin film evaporator for evaporation, feeding the refined horse oil ethyl ester into a light component kettle, and introducing nitrogen for protection.
2. The process of claim 1, wherein in step b, absolute ethanol and alkali are sequentially added to the esterification reaction kettle, the mixture is heated and stirred, the alkali is completely dissolved in the absolute ethanol, and then the crude horse oil is added.
3. The production process of refined horse oil ethyl ester according to claim 1, wherein in step b, after the esterification reaction is completed, the vertical condenser is closed, the horizontal condenser is opened, and the anhydrous ethanol is recovered by a reduced pressure distillation method at 70-72 ℃.
4. The process of claim 1, wherein in step c, crude horse oil ethyl ester is added to 2/3 of the volume of the heavy ends kettle.
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| CN101766238A (en) * | 2009-12-31 | 2010-07-07 | 山东三星玉米产业科技有限公司 | DHA-based corn oil for children only and method for preparing the same |
| CN102277228A (en) * | 2011-07-18 | 2011-12-14 | 中国科学院成都生物研究所 | Preparation method and application of refined ostrich oil |
| CN103509651A (en) * | 2012-06-27 | 2014-01-15 | 浙江海洋学院 | Method for extracting ethyl ester enriched fish oil from fish oil refining byproduct |
| CN104974857A (en) * | 2015-06-30 | 2015-10-14 | 新疆农业大学 | Method for preparing horse oil through ethyl esterification and prepared horse oil |
| CN106281723A (en) * | 2016-08-31 | 2017-01-04 | 菏泽尧舜牡丹生物科技有限公司 | A kind of high ethyl esterified technique of acid value peony seed oil |
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| FR2991337B1 (en) * | 2012-05-29 | 2016-09-02 | Roquette Freres | CONTINUOUS PROCESS FOR ENRICHING DHA WITH ETHYL ESTERS OF AN OIL PRODUCED BY MICROALGUES |
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| CN101766238A (en) * | 2009-12-31 | 2010-07-07 | 山东三星玉米产业科技有限公司 | DHA-based corn oil for children only and method for preparing the same |
| CN102277228A (en) * | 2011-07-18 | 2011-12-14 | 中国科学院成都生物研究所 | Preparation method and application of refined ostrich oil |
| CN103509651A (en) * | 2012-06-27 | 2014-01-15 | 浙江海洋学院 | Method for extracting ethyl ester enriched fish oil from fish oil refining byproduct |
| CN104974857A (en) * | 2015-06-30 | 2015-10-14 | 新疆农业大学 | Method for preparing horse oil through ethyl esterification and prepared horse oil |
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